CN105080448B - Millimeter channel type continuous preparation system - Google Patents
Millimeter channel type continuous preparation system Download PDFInfo
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- CN105080448B CN105080448B CN201510570927.3A CN201510570927A CN105080448B CN 105080448 B CN105080448 B CN 105080448B CN 201510570927 A CN201510570927 A CN 201510570927A CN 105080448 B CN105080448 B CN 105080448B
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Abstract
The invention provides a millimeter channel type continuous preparation system which can be used in preparation of various inorganic nonmetal nanocrystallines (such as oxides and sulfides). Compared with the prior art, the system has the advantages that 1, a millimeter channel type reaction pipe is adopted, and is internally provided with inner threads, so that turbulent flows are promoted to be generated in the channel, and heat and mass transfer is promoted effectively in the channel; 2, an ultrafiltration purification device is adopted for filtering out raw material molecules or ions which are subjected to non-complete reaction in a reaction mixed liquid, so that the continuous preparation of products is realized; 3, if a material tank is improved further, nitrogen can be introduced, so that the materials can be isolated from oxygen at the normal temperature, and channel type heat reaction is realized under an inert atmosphere. The millimeter channel type continuous preparation system can be used for the pilot plant test preparation of the nanocrystallines and high-molecular polymers, and can be used for effectively controlling the sizes or the molecular weight distribution of the materials.
Description
Technical field
Pilot scale reaction preparation system technical field is prepared the present invention relates to nanocrystalline or polymer serialization, is specifically related to
And a kind of millimeter channel-type serialization preparation system.
Background technology
The physicochemical characteristics of semiconductor nano, the molecular weight of organic high molecular polymer or Size Distribution for material
With important influence.Traditional reactor has that heat and mass effect is poor in Large Copacity preparation process, it is impossible to enough
Effectively control the molecular weight or Size Distribution of material.In order to further improve the combined coefficient and synthesis quality of material, using micro-
Channel reactor turns into focus of concern.Famous company and research institution in the world, such as Du Pont, the Massachusetts Institute of Technology,
Hereby microtechnology research institute, BASF, Merck, Schering, Bayer etc. are all engaged in positive to Mainz in terms of micro-reacting tcchnology
Research.Can be efficiently against many weak points of traditional reactor, in Large Copacity preparation process using micro passage reaction
Show that specific surface area is high, take up an area less, mass-and heat-transfer effect is good, the plurality of advantages that can be continuously produced.Even so, microchannel
Reactor processing cost is sufficiently expensive, product flow is very low and pipeline is easily blocked, and many will be faced in actual applications and is asked
Topic.
The content of the invention
The present invention regarding to the issue above, proposes that a kind of preparation for nanocrystalline or polymer millimeter channel-type serialization is
System, with reference to internal thread is set in passage, promotes to form turbulent flow, strengthens the heat and mass transfer process in passage, is ensureing to react
While journey has excellent mass-and heat-transfer performance, the blocking of reaction channel is prevented.Also, device is purified by ultrafiltration to filter instead
The raw molecule or ion not reacted completely in mixed liquor are answered, realizes prepared by the serialization of the products such as nanocrystalline or polymer.
To realize object above, this invention takes following technical scheme：
A kind of millimeter channel-type serialization preparation system, including head tank 1, peristaltic pump 2, channel-type reaction tube 3, condenser pipe
5th, surge tank 7, peristaltic pump 8 and ultrafiltration apparatus 9；The output end of head tank 1 is connected (former with the input of peristaltic pump 2 by pipeline
Batch can 1 is additionally provided with charge door in addition to output end, for adding raw material), the output end of peristaltic pump 2 passes through pipeline and channel-type
The input connection of reaction tube 3；The internal diameter of channel-type reaction tube 3 is 1~10mm, and temperature control is uneven if aperture is more than 10mm
Even, less than 1mm, then temperature is easily blocked；The length of channel-type reaction tube 3 is not limited, depending on being needed according to reaction；Channel-type
The inwall of reaction tube 3 is provided with internal thread, and pitch is preferably 1~5mm, can promote uniform mass transfer；Such as need to control reaction temperature
System regulation, channel-type reaction tube 3 can be placed in temperature regulating device, such as water bath device, oil bath device etc.；Channel-type reaction tube 3
Output end be connected with the input of condenser pipe 5 by pipeline, cooled down by the reactant in condenser pipe, reach termination
The purpose of reaction；For general reaction, directly can be cooled down toward being passed through running water in condenser pipe, it is also possible to use recirculated water
Cooling device is bathed to obtain specific condensation temperature；The output end of condenser pipe 5 is connected by pipeline with the input of surge tank 7,
The output end of surge tank 7 is connected by pipeline with the input of peristaltic pump 8；The output end of peristaltic pump 8 is filled by pipeline with ultrafiltration
Put 9 input connection；The effect of surge tank 7 is, flow velocity of the reaction solution in channel-type reaction tube 3 with ultrafiltration apparatus
Flow velocity and pressure it is different, therefore reaction solution needs to be introduced into surge tank and stops, then is input into ultrafiltration apparatus 9 by peristaltic pump 8
In.Ultrafiltration apparatus 9 can be small under the pressure that peristaltic pump 8 is provided using hollow tubular type, after reaction solution is passed through ultrafiltration apparatus 9
Molecule is discharged by the filter membrane in device, and product is retained in reaction solution；Such as, following structure can be used：Including inner tube
901st, outer tube 902 and filter membrane 903, filter membrane 903 are arranged between inner tube 901 and outer tube 902, contain solvent in outer tube 902, when anti-
When answering liquid to flow through inner tube 901, under the pressure that peristaltic pump 8 is provided, size is less than the ion in the aperture of filter membrane 903, molecule through filter
Film 903 enters outer tube 902, and semiconductor nano or polymer beads are retained in the reaction solution in inner tube 901, from ultrafiltration
The output end outflow of device 9, plays the purpose of ultrafiltration purification, so as to realize prepared by nanocrystalline or polymer serialization.It is super
Filter sizes in filter device 9 are selected according to the nanocrystalline size that target synthesizes, to be defined less than synthesized nanocrystalline size,
Typically usable 1nm~10nm, it is ensured that the complete inorganic ions of unreacted retains the products such as semiconductor nano through removal.
Can be by the further improvement to head tank, with suitable for different reaction conditions.One of which is improved as follows：
Head tank 1 includes tank body 11, heater 12, agitator 13, aspiration pump 14, air accumulator 15, the top of tank body 11 set air inlet 16,
Bleeding point 17, temperature-measuring port 18 and charge door 19, bleeding point 17 are connected with aspiration pump 14, and air inlet 16 is connected with air accumulator 15, survey
Warm device measures the temperature in tank body and controls heater 12 by temperature-measuring port 18.Wherein, heater 12, temperature-measuring port 18 and thermometric
Device is used to monitor the temperature of head tank, and monitoring temperature is not needed such as, can remove.And if reaction condition does not need indifferent gas
Atmosphere, then aspiration pump 14, air accumulator 15, air inlet 16, bleeding point 17 can remove.Optimization, head tank is also provided with pressure
Control device, in case tank interior pressure exceedes setting value；Such as, gas outlet can be set, gas outlet is connected by pipeline with oil sealing
Connect, when air pressure is more than 1 atmospheric pressure in tank, gas is overflowed by oil-sealing arrangement, prevents overvoltage.
Channel-type reaction tube 3 can mainly be existed using conventional shape, such as helix tube type or straight pipe type, the selection of shape
In the occupancy in device space, the Area comparison that helix tube type takes is few, more often uses, but it is also possible to use straight pipe type, to invention
Effect do not influence；The material of channel-type reaction tube 3 is not particularly limited, can be resistance to from metal, glass, quartz or heatproof
The conventional material such as solvent plastics (such as polytetrafluoroethylene (PTFE) or PolyTHF), typically according to reaction condition or the property of product
Matter selects suitable material.
Further, the serialization of multistep reaction can be realized by being sequentially connected in series several preparation systems of the present invention.
The feasible serial connection method of one of which is that first output end of the ultrafiltration apparatus of preparation system 9 is by pipe
Road can be directly with second preparation system head tank be connected, product that first preparation system is obtained and second system
Second step reaction is carried out after raw material mixing in head tank.
Several preparation systems of the present invention can also be carried out parallel connection, improve the efficiency of reaction, it is also possible to realized in difference
Reacted while reaction condition.
The feasible parallel method of one of which is：Multiple preparation systems use same head tank 1, are drawn from head tank 1
A plurality of pipeline is connected with the peristaltic pump 2 of each system respectively.
Millimeter channel-type serialization preparation system of the invention can be used to being prepared under certain reaction temperature various inorganic non-
Metallic nano crystal (such as oxide, sulfide).Can be used to nanocrystalline, high molecular polymer pilot scale prepare, effectively control material
The size or molecular weight distribution of material.The present invention compared with prior art, has the following advantages that：
1st, using grade channel-type reaction tube, and internal thread is set, promotes turbulent flow in passage, effectively facilitate passage
Interior heat and mass；
2nd, it is purified by ultrafiltration device and filters the raw molecule or ion not reacted completely in reaction mixture, realizes producing
It is prepared by the serialization of thing；
If the 3, head tank can be passed through nitrogen by further improvement, make raw material starvation at normal temperatures, realize in inertia
Channel-type heating response under atmosphere.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is the structural representation of embodiment 1；
Fig. 3 is channel-type reaction tube cross-sectional view；
Fig. 4 is ultrafiltration apparatus structural representation；
Fig. 5 is the structural representation of head tank after improving；
Fig. 6 is embodiment 1CuInS2Nanocrystalline transmission electron microscope photo；
Fig. 7 is embodiment 2CuInS2The transmission electron microscope photo of/ZnS nanocrystalline；
Fig. 8 is comparative example 1CuInS2Nanocrystalline transmission electron microscope photo；
Fig. 9 is comparative example 2CuInS2Nanocrystalline transmission electron microscope photo.
Wherein：1, head tank；2, peristaltic pump；3, channel-type reaction tube；4, oil bath device；5, condenser pipe；6, circulator bath
Cooling device；7, surge tank；8, peristaltic pump；9, ultrafiltration apparatus；11, raw material tank；12, heater；13, agitator；14, take out
Air pump；15, air accumulator；16, air inlet；17, bleeding point；18, temperature-measuring port；19, charge door；901, inner tube；902, outer tube；903,
Filter membrane.
Specific embodiment
Present disclosure is described in further details with reference to the accompanying drawings and detailed description.
Embodiment 1
The preparation system that the present embodiment is used is as shown in Fig. 2 specific as follows：
The output end of head tank 1 is connected by pipeline with the input of peristaltic pump 2, and the output end of peristaltic pump 2 passes through pipeline
Input with channel-type reaction tube 3 is connected；Channel-type reaction tube 3 is arranged in oil bath device 4, and oil bath device 4 act as
Reaction temperature of the control passage formula reaction tube 3 in setting；Channel-type reaction tube 3 is helix tube type, and internal diameter is 6mm, length is
27m, inwall is provided with internal thread (as shown in Figure 3), and pitch is 1mm, can promote uniform mass transfer；The output of channel-type reaction tube 3
End is connected by pipeline with the input of condenser pipe 5, the reactant in condenser pipe is carried out using circulator bath cooling device 6 cold
But, the purpose of terminating reaction is reached；The output end of condenser pipe 5 is connected by pipeline with the input of surge tank 7, surge tank 7
Output end is connected by pipeline with the input of peristaltic pump 8, and the output end of peristaltic pump 8 passes through the input of pipeline and ultrafiltration apparatus 9
End connection.The structure of ultrafiltration apparatus 9 is as shown in figure 4, including inner tube 901, outer tube 902 and filter membrane 903, filter membrane 903 is arranged at interior
Between pipe 901 and outer tube 902, filter sizes are 2nm；White arrow represents the flow direction of reaction solution, and black arrow represents small
Molecule through filter membrane direction；Contain solvent in outer tube 902, reaction solution from peristaltic pump 8 out after, by the defeated of ultrafiltration apparatus 9
Enter end and enter inner tube 901, under the pressure that peristaltic pump 8 is provided, size is less than the ion in the aperture of filter membrane 903, molecule and passes through filter membrane
903 enter outer tube 902, and the size of product is retained in the reaction solution in inner tube 901, through ultrafiltration more than the aperture of filter membrane 903
The output end outflow of device 9.
The head tank of the device carries out following improvement so that the materials synthesis that the device is used under inert atmosphere：Such as Fig. 5
Shown, improved head tank includes tank body 11, heater 12, agitator 13, aspiration pump 14, air accumulator 15, and the top of tank body 11 sets
Air inlet 16, bleeding point 17, temperature-measuring port 18 and charge door 19 (also having output end, but no display in Figure 5 on tank body 11) are put,
Bleeding point 17 is connected with aspiration pump 14, and air inlet 16 is connected with air accumulator 15, and temperature measuring equipment is measured in tank body by temperature-measuring port 18
Temperature and control heater 12.Further, pressure control device is also provided with, in case tank interior pressure exceedes setting
Value.
CuInS2Nanocrystalline preparation：
1st, 19.1g cuprous iodides, 29.2g indium acetates, 1000ml n- dodecyl mereaptans are added into head tank 1 from charge door 19
In tank body 11, then start aspiration pump 14 and vacuumize 5min, after stopping pumping, nitrogen 5min is passed through from air accumulator 15, grasp repeatedly
Make 3 times, then, the temperature in tank body 11 is risen to 100 DEG C by heater 12, mixed solution to clarification is stirred at 100 DEG C；
2nd, the flow velocity for setting peristaltic pump 2 is 33ml/min, and the temperature of oil bath device 4 is set as 220 DEG C, when the temperature of oil bath device 4
When degree reaches design temperature, start peristaltic pump 2, will be reacted in head tank 1 reaction solution input channel formula reaction tube 3,
Product flows out from channel-type reaction tube 3 after about 10min；
3rd, the product out of channel-type reaction tube 3 is during first condensed pipe 5 is cooled down and flows into surge tank 7, terminating reaction；
4th, the flow velocity for setting peristaltic pump 8 is 5ml/min, and reaction solution pumps into ultrafiltration apparatus 9 by peristaltic pump 8, and efflux is
It is CuInS after purification2Nanocrystal solution.
Prepared CuInS2Nanocrystalline even size distribution, good dispersion.Fig. 6 is prepared CuInS2Nanocrystalline is saturating
Electromicroscopic photograph is penetrated, average grain diameter is 2.5nm or so.
Embodiment 2
As different from Example 1, two millimeter channel-type serialization preparation systems are used in series in the present embodiment, can be used
In the synthesis of nano-crystal with core-shell structure.The present embodiment is with CuInS2The preparation of/ZnS nanocrystalline is specifically described：
First preparation system is same as Example 1；Second preparation system and first preparation system difference exist
In the internal diameter of, channel-type reaction tube 3 be 6mm, length be 81m, internal thread pitch is 5mm.
The step of the step of the present embodiment preparation process 1~4, uses first preparation system, concrete operations and embodiment 11
~4 is identical.
5th, the CuInS for obtaining first preparation system2Nanocrystal solution is directly added into second raw material of preparation system
In tank (afterwards in the description of the present embodiment, all component all refers to second component of preparation system), and add 202.4g ten
Four alkanoic acid zinc, 800ml octadecylenes, then start aspiration pump 14 and vacuumize 5min, after stopping pumping, nitrogen are passed through from air accumulator 15
5min, is operated 3 times repeatedly, then, the temperature in tank body 11 is risen into 100 DEG C by heater 12, and mixing is stirred at 100 DEG C
Solution is extremely clarified；
6 and the flow velocity of peristaltic pump 2 is set for 33ml/min, the temperature of oil bath device 4 is set as 230 DEG C, works as oil bath device
When 4 temperature reach design temperature, start peristaltic pump 2, will be carried out in head tank 1 reaction solution input channel formula reaction tube 3 anti-
Should, product flows out from channel-type reaction tube 3 after about 30min；
7th, the product out of channel-type reaction tube 3 is during first condensed pipe 5 is cooled down and flows into surge tank 7, terminating reaction；
8th, the flow velocity for setting peristaltic pump 8 is 5ml/min, and reaction solution pumps into ultrafiltration apparatus 9 by peristaltic pump 8, and efflux is
It is CuInS after purification2/ ZnS nanocrystalline solution.
Prepared CuInS2/ ZnS nanocrystalline even size distribution, good dispersion.Fig. 7 is prepared CuInS2/ ZnS receives
The transmission electron microscope photo of meter Jing, average grain diameter is 3.7nm or so.
Embodiment 3
The internal diameter of channel-type reaction tube 3 is 10mm as different from Example 1.The size of products therefrom, uniformity, dispersion
Property is same as Example 1.
Embodiment 4
The internal diameter of channel-type reaction tube 3 is 1mm as different from Example 1.The size of products therefrom, uniformity, dispersion
Property is same as Example 1.
Comparative example 1
Compared with Example 1, difference is that channel-type tube inner diameter is 10mm, does not use internal thread.It is made
Standby CuInS2Nanocrystalline Size Distribution is uneven.Fig. 8 is prepared CuInS2Nanocrystalline transmission electron microscope photo.
Comparative example 2
Compared with Example 1, channel-type tube inner diameter is 0.5mm.In preparation process, pipeline is blocked, and made
Standby nano particle is reunited, and Fig. 9 is prepared CuInS2Nanocrystalline transmission electron microscope photo.
Claims (3)
1. a kind of millimeter channel-type serialization preparation system, it is characterised in that including head tank (1), peristaltic pump (2), channel-type
Reaction tube (3), condenser pipe (5), surge tank (7), peristaltic pump (8) and ultrafiltration apparatus (9)；The output end of head tank (1) is by pipe
Road is connected with the input of peristaltic pump (2), and the output end of peristaltic pump (2) is by pipeline and the input of channel-type reaction tube (3)
Connection；The internal diameter of channel-type reaction tube (3) is 1~10mm, and inwall is provided with internal thread；The pitch of the internal thread be 1~
5mm；The output end of channel-type reaction tube (3) is connected by pipeline with the input of condenser pipe (5)；The output end of condenser pipe (5)
It is connected with the input of surge tank (7) by pipeline, the output end of surge tank (7) is by pipeline and the input of peristaltic pump (8)
Connection, the output end of peristaltic pump (8) is connected by pipeline with the input of ultrafiltration apparatus (9)；During the ultrafiltration apparatus (9) use
Empty tubular structure, including inner tube (901), outer tube (902) and filter membrane (903), filter membrane (903) are arranged at inner tube (901) and outer tube
(902) between, the two ends of inner tube (901) connect with the input and output end of ultrafiltration apparatus (9) respectively.
2. as claimed in claim 1 millimeter of channel-type serialization preparation system, it is characterised in that the head tank (1) includes
Tank body (11), heater (12), agitator (13), aspiration pump (14), air accumulator (15), tank body (11) top set air inlet
(16), bleeding point (17), temperature-measuring port (18) and charge door (19), bleeding point (17) are connected with aspiration pump (14), air inlet (16)
It is connected with air accumulator (15).
3. as claimed in claim 1 or 2 millimeter of channel-type serialization preparation system, it is characterised in that the channel-type reaction
Pipe (3) is helix tube type or straight pipe type.
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| CN106916584B (en) * | 2017-04-21 | 2018-06-15 | 东莞市睿泰涂布科技有限公司 | Quantum dot synthesizer and quantum dot synthetic method |
| WO2018192539A1 (en) * | 2017-04-21 | 2018-10-25 | 东莞市睿泰涂布科技有限公司 | Quantum dot core synthesis device and quantum dot core synthesis method |
| WO2018192540A1 (en) * | 2017-04-21 | 2018-10-25 | 东莞市睿泰涂布科技有限公司 | Quantum dot core-shell synthesis device and quantum dot core-shell synthesis method |
| WO2018192541A1 (en) * | 2017-04-21 | 2018-10-25 | 东莞市睿泰涂布科技有限公司 | Quantum dot precursor synthesis device and quantum dot precursor synthesis method |
| CN106914208B (en) * | 2017-04-21 | 2018-06-15 | 东莞市睿泰涂布科技有限公司 | Quantum dot precursor synthesis device and quantum dot precursor synthesis method |
| CN113588851B (en) * | 2021-07-28 | 2023-06-09 | 福建中烟工业有限责任公司 | Method for extracting and measuring dithiocarbamic acid ester, measuring device and application thereof |
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| CN101565175A (en) * | 2009-06-05 | 2009-10-28 | 华东理工大学 | Device of fast synthetizing CdSe quantum dots and method thereof |
| US20150030531A1 (en) * | 2012-03-12 | 2015-01-29 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Operation method for multichannel apparatus and multichannel apparatus |
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